Identification and quantification of the main organic components of vinegars by high resolution 1H NMR spectroscopy |
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Authors: | Caligiani A Acquotti D Palla G Bocchi V |
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Affiliation: | a Dipartimento di Chimica Organica e Industriale, Università degli Studi di Parma, Via Usberti 17A, 43100-Parma, Italy b Centro Interfacoltà Misure, Università degli Studi di Parma, Via Usberti 23A, 43100-Parma, Italy |
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Abstract: | A detailed analysis of the proton high-field NMR spectra of vinegars (in particular of Italian balsamic vinegars) is reported. A large number of organic substances belonging to different classes, such as carbohydrates, alcohols, organic acids, volatile compounds and amino acids, were assigned. The possibility of quantification of the substances identified in the whole vinegar sample, without extraction or pre-concentration steps, was also tested. The data validity was demonstrated in terms of precision, accuracy, repeatability and inter-day reproducibility. The effects of the most critical experimental parameters (sample concentration, water suppression and relaxation time) on the analysis response were also discussed. 1H NMR results were compared with those obtained by traditional techniques (GC-MS, titrations), and good correlations were obtained. The results showed that 1H NMR with water suppression allows a rapid, simultaneous determination of carbohydrates (glucose and fructose), organic acids (acetic, formic, lactic, malic, citric, succinic and tartaric acids), alcohols and polyols (ethanol, acetoin, 2,3-butanediol, hydroxymethylfurfural), and volatile substances (ethyl acetate) in vinegar samples. On the contrary, the amino acid determination without sample pre-concentration was critical. The 1H NMR method proposed was applied to different samples of vinegars, allowing, in particular, the discrimination of vinegars and balsamic vinegars. |
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Keywords: | Quantitative analysis 1H NMR Vinegars Balsamic vinegars |
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